JPS5812267B2 - Manufacturing method of metal settsuken - Google Patents

Abstract

The invention relates to a method for producing metal soaps by reacting aliphatic carboxylic acids with metal oxides, metal hydroxides and/or metal carbonates, wherein the metal soaps are directly obtained in the form of granulates without requiring an additional granulating step.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to at least one aliphatic carboxylic acid having about 8 to 22 carbon atoms, and at least one metal oxide and/or metal hydroxide and/or metal carbonate. The present invention relates to a method for producing a metal soap or a metal soap mixture by reacting a salt with a salt in the presence of water at elevated temperature and stirring, and then removing water.

Conventionally, a method for obtaining metal soaps by a two-step reaction of carboxylic acids has been known.

A first stage reaction with an equal volume of sodium hydroxide solution or potassium hydroxide solution gives the corresponding alkaline soaps.

In the next step, when this alkaline soap is mixed with the selected metal salt, an insoluble metal salt is formed and precipitated.

The reaction is carried out at a temperature of 60-70° C. in the presence of about 20 times the amount of water relative to the acid used.

Separation of the precipitated metal soap is carried out, for example, by phosphor filtration or centrifugation.

At the same time, the proportion of alkali salts formed is reduced to less than 1% by washing with water, and the metal soap is dried and pulverized.

The final product is in a bulky form with very low density, and a particular disadvantage that must be considered is the generation of large amounts of dust.

Another drawback of this method is that it requires multiple steps.

Other known methods involve reacting carboxylic acids with the corresponding metal oxides, hydroxides or carbonates under melt conditions.

In this method, a metal oxide, hydroxide, or carbonate is added to a molten carboxylic acid at a temperature above the expected melting point of the final product, and the resulting water of reaction and water of hydration is evaporated. This is to remove it.

The anhydrous melt is then solidified using a cooling tower, cooling cylinder or cooling bath and then ground.

The disadvantage of this method is that it also produces dust and the desired product has a rather dark tinge.

Furthermore, the processing of this product is particularly hampered by the coarse particles and therefore the insufficient distribution.

DE-As 1068238 describes a method for producing lead salts of fatty acids.

According to this universal method, the reaction of granular or finely powdered fatty acids with lead oxide is carried out in an aqueous suspension at a temperature slightly below the melting temperature of the acid.

The obtained insoluble lead mixture is suction filtered and dried.

The disadvantage of this method lies in the amount of water required to distribute the fatty acids as a fine powder in an aqueous suspension, which is about 6 to 13 times the amount of carboxylic acid used. .

With this method, the final product cannot be obtained directly in granular form.

The object of the invention is to overcome the drawbacks of the conventional methods and to produce metal soaps or metal soap mixtures directly in granular form substantially dust-free, simply and economically, without special processing steps. [The purpose is to provide an improved manufacturing method that can be obtained.

According to the invention, said object is achieved in the method described at the outset by adding 1 to 5% of water relative to the total weight of the carboxylic acid(s) and heating the mixture to the temperature required to initiate the reaction. This is accomplished by allowing the exothermic reaction to proceed in a closed reactor without external heating, then reducing the overpressure generated, and draining the water contained in the reaction mixture under reduced pressure.

The method of the present invention has the following advantages over conventional methods.

A particular disadvantage of the conventional process is that the target product has a high dust content and a somewhat dark tinge.

In the process of the invention it is surprisingly possible to obtain the desired product directly in granular form.

The product therefore does not generate substantial amounts of dust and exhibits improved properties compared to metal soaps obtained by two-step reaction in the aqueous phase or by direct reaction in the melt.

The particle size distribution of the target product obtained in granular form by the process of the invention is very favorable, since about 80% of the total amount lies in the desired particle size range.

Thus, for example, the process according to the invention makes it possible to obtain a product in which about 80% of the metal particles are in the particle size range of 0.2 mm to 2 mm.

Another advantage of the process according to the invention over the conventional methods is that energy can be saved and the reaction as well as the subsequent drying step are therefore more economical than the conventional methods.

This means that in the conventional method, 2 times the amount of carboxylic acid used.
It is necessary to heat 0 times the amount of water, and there is no need to add special energy to dry metal soap using the method of the present invention, that is, the amount of heat contained in the reactor contents exceeds that of the reactor. This is because it is sufficient to completely evaporate water during exhaust.

Furthermore, in the known two-stage reaction process mentioned above, the drying of the metal soaps is carried out by conventional drying methods (e.g. belt dryer, fluidized bed dryer, tray dryer, drum dryer, cascade dryer 7), Environmental pollution occurs due to the release of extremely fine dust particles.

According to the method of the invention, the production of the metal soap or metal soap mixture by the reaction leading to the desired product takes place in a closed container.

It is therefore simpler and less time consuming than conventional methods.

Preferred embodiments of the method of the invention are as follows.

an aliphatic carboxylic acid having about 8 to 22 carbon atoms and/or a mixture of the acids in a pressurized reaction vessel with at least one metal oxide and/or hydroxide and/or carbonate;
Carboxylic acid (1 to 5% based on the total weight of one type or mixture)
of water is added and mixed, then the mixture is heated to the temperature required to initiate the reaction.

The mixture is stirred while the exothermic reaction proceeds at a temperature of about 90-110°C.

At this time, the internal pressure is approximately 1.1 to 1.1 for approximately 10 to 15 minutes.
It reaches 1.3 bar.

After the reaction is completed, the generated pressure is reduced, and the added water and the water produced by the reaction are extracted under reduced pressure conditions, preferably while increasing the stirring speed.

This allows the temperature of the reaction product to drop relatively quickly to about 50 DEG -55 DEG C., and the desired product is obtained in granular form.

The resulting granules are screened and the undesired coarse and fine particles (which only represent about 10% of the total amount) are returned to the next reaction mixture.

In the method according to the invention, the amount of water added is preferably 2 to 4% based on the total amount of carboxylic acid (one type or a mixture), since this provides optimum results.

In order to initiate the exothermic reaction in the process of the invention, activation energy must first be applied in the form of heating.

In this regard, the mixture should be at least up to the melting point of the carboxylic acid used or at least up to the melting range of the carboxylic acid mixture used, i.e. generally about 50 to 60
It has been found that heating to 0.degree. C. is particularly preferred.

The aliphatic carboxylic acid having about 8 to 22 carbon atoms is preferably selected from linear carboxylic acids which may contain a hydroxyl group.

In order to obtain the colorless target product, the process according to the invention requires lithium, sodium, potassium, magnesium, calcium, cadmium, strontium, barium, tin,
Preference is given to using oxides and/or hydroxides and/or carbonates of metals selected from the group consisting of lead and zinc.

However, it is also possible to use oxides and/or hydroxides and/or carbonates of metals selected from the group consisting of copper, iron, nickel, manganese and chromium; The metal sets used are colored and are therefore generally less desirable.

Metal oxides and/or hydroxides and (
or) It is preferable that the amount of carbonate used is at least equal to the amount of acid used.

After the reaction, at least one metal oxide and/or
It is even more preferred to use about 2% excess of hydroxide and/or carbonate over equivalent amounts to acid.

When metal soap produced by conventional methods is made into granules, a granulating additive is added to the metal soap in a high-speed mixer or granulator, and the mixture is granulated at a temperature higher than the melting point of the additive. ,
Additional steps of cooling and sieving are required.

However, with the method of the present invention, it is possible to directly obtain granules that are soft, have good flowability, and can be easily formulated.

Therefore, if desired, the obtained granular metal soap can be drained using, for example, a known lubricant (such as paraffins or oils) that is normally used as a granulation additive, and then the same Coating can be done within the reactor.

Specific examples of the present invention will be explained in detail with reference to the following examples.

Example 1 The production chain length of calcium soap was C14 to C2o (C2o2%, C1364%, C
172%, C1628%, C144%) with an average molecular weight of 273 are charged into a pressurized reactor with a capacity of 130 l equipped with a stirrer together with 0.5 l water and 3.5 kg calcium hydrate. .

When the mixture is heated to 50-60<0>C, the reaction proceeds exothermically and no heating is necessary.

If the reaction continues with stirring, the pressure inside the closed reactor will be 1.
rises to 1-1.3 bar.

The reaction ends when the pressure or temperature begins to decrease.

The reaction vessel is then evacuated and the water contained is drawn off under reduced pressure while stirring is continued.

The target product obtained directly in this way is granular;
Free-flowing, with a narrow particle size distribution? It is a calcium supplement that does not contain any minerals.

The following examples were carried out in the same manner as Example 1.

Example 2 Preparation of lead soap 25 g of the same carboxylic acid mixture as in Example 1 is reacted with 0.5 l of water and 10.6 kg of lead oxide.

Example 3 Production of Zinc Sedaken 25 kg of the same carboxylic acid mixture as in Example 1 was added to 0.5 liters of water.
and 3.75 kg of zinc oxide.

Example 4 Production of barium-strength domium soap Chain length cto xc1, (cto 1%, C193%
, CO46%) with an average molecular weight of 200, 0.5 l of water, and 4.0 cadmium oxide.
kg and 5.4 kg of barium hydroxide.

Example 5 Production of barium-cadmium liquid 25 kg of the same carboxylic acid mixture as in Example 1 was added to 0.0 ml of water.
5J, cadmium oxide2. 9 5 F and 2.95 kg of barium hydroxide.

Example 6 Production of sodium soap 30 kg of the same carboxylic acid mixture as in Example 1 was added to 0.0 kg of water.
5J and sodium hydroxide (100% purity) 4.4kg
react with.

Example 7 Manufacture of barium soap 30 kg of the same carboxylic acid mixture as in Example 1 was added to 0.0 kg of water.
5l and barium hydroxide9. React with 5 kg.

In Examples 2-7 as well, the products obtained were free-flowing, particulate dust-free metal soaps.

Claims (1)

[Scope of Claims] 1. At least one aliphatic carboxylic acid having about 8 to 22 carbon atoms, and at least one metal oxide and/or metal hydroxide and/or metal carbonate; In the method of producing a metal soap mixture by reacting in the presence of water at elevated temperature and stirring, and then removing water, based on the total weight of the carboxylic acid (one type or mixture). The reaction is started by adding 1-5% water and heating the reaction mixture to at least the melting point of the carboxylic acid used or at least the melting range of the carboxylic acid mixture used, in a closed reactor, It is characterized by allowing the exothermic reaction to proceed without heating, and after the completion of the reaction, reducing the overpressure generated and removing the water contained in the reaction product under reduced pressure to directly obtain granular metal soap. how to. 2 Based on the total weight of carboxylic acid (one type or mixture),
The method according to claim 1, characterized in that 2 to 4% of water is added. 3. Claim 1, characterized in that the carboxylic acid (one type or mixture) having about 8 to 22 carbon atoms used is selected from linear carboxylic acids that may contain a hydroxyl group. The method described in Section 1 or Section 2. 4 Lithium, sodium, potassium, magnesium,
Calcium, cadmium, strontium, barium,
Claims 1 to 3 are characterized in that at least one oxide and/or hydroxide and/or carbonate of a metal selected from the group consisting of tin, lead and zinc is used. The method according to any one of paragraph 3. 5. Any one of claims 1 to 4, characterized in that the amount of metal oxide and/or hydroxide and/or carbonate used is at least equivalent to the amount of acid. The method described in Section 1. 6. At least one metal oxide and/or hydroxide and/or carbonate is used in approximately 2% excess of the equivalent amount relative to the carboxylic acid. The method according to any one of items 1 to 4.